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The NbCl 5  adducts of M[NbCl 6 ] · NbCl 5  with M = K or NO are structurally related via their common super group  Fmmm . K[NbCl 6 ] · NbCl 5  crys tallizes in the triclinic space group  C -1 with  a  = 9.898(1),  b  = 9.443(1),  c  = 17.370(1) Å,  α  = 89.57(1),  β  = 108.49(1),  γ  = 90.54(1)° and  Z  = 4 at room temperature. For the mono clinic nitrosonium compound with space group  C 2/ c  X-ray diffraction data have been recorded at 173 K giving  a  = 9.530(1),  b  = 9.412(1),  c  = 33.38(1) Å,  β  = 92.68(1)° and  Z  = 8. Layers of NbCl 5  dimers alternate with cation-centred double layers of the NbCl 6  –  ions, oriented parallel to the  a – b  plane. Com pared to the cubic perovskite SrTiO 3 , the NbCl 6  –  ‘octahedra’ of the K +  salt are uniformly rotated by 5° around the stack ing axis. On the contrary, the NO +  salt shows ‘antiferrorotative’ ordering by ±12° in alternate layers. Crystal symmetry and twinning laws reflect the structural differences, but the similarity between both structures prevails.

The crystal structures of K[NbCl 6 ] · NbCl 5 and NO[NbCl 6 ] · NbCl 5